CN110004522A - A kind of porous carbon fiber material and its preparation method and application - Google Patents

A kind of porous carbon fiber material and its preparation method and application Download PDF

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Publication number
CN110004522A
CN110004522A CN201910268603.2A CN201910268603A CN110004522A CN 110004522 A CN110004522 A CN 110004522A CN 201910268603 A CN201910268603 A CN 201910268603A CN 110004522 A CN110004522 A CN 110004522A
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CN
China
Prior art keywords
carbon fiber
porous carbon
liner
fiber material
tank body
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Withdrawn
Application number
CN201910268603.2A
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Chinese (zh)
Inventor
戴军
于帮龙
杨莉
张尧成
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Changshu Institute of Technology
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Changshu Institute of Technology
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Publication date
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Priority to CN201910268603.2A priority Critical patent/CN110004522A/en
Publication of CN110004522A publication Critical patent/CN110004522A/en
Withdrawn legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate

Abstract

The present invention provides a kind of preparation methods of porous carbon fiber material, it is base stock by using draft fasciated fiber, charing obtains porous carbon fiber in an inert atmosphere, draft fasciated fiber is impregnated by sodium chloride solution simultaneously, increase carbon fibre material toughness, resulting carbon fibre material merging, which is equipped with heating oil and is filled in the pressure pan of inert atmosphere, impregnates, and heating oil is then warming up to 150 DEG C -230 DEG C with the heating rate of 6-10 DEG C/min, constant temperature 1-3h, while pressure pan rotates；It is placed in high temperature furnace after the resulting carbon fibre material of step S3 is taken out; 750 DEG C -880 DEG C are warming up under inert atmosphere protection with the heating rate of 8-14 DEG C/min; then constant temperature 3-5h carries out activation etching; high-pressure steam is sprayed to carbon fibre material in 1/3 and 2/3 timing node of heating; it forms carbon fibre material more porous, avoids being fabricated to basic fibrous raw material using industrial chemicals, reduce the use of industrial chemicals; the energy has been saved, environmental pollution is avoided.

Description

A kind of porous carbon fiber material and its preparation method and application
Technical field
The present invention relates to field of material technology, in particular to a kind of porous carbon fiber material and its preparation method and application.
Background technique
In recent years, porous carbon section causes increasingly extensive concern in materials science field, this is because porous carbon It is controllable and reasonable layout micropore, mesoporous and macropore ternary nano pore structure that material, which has both aperture, has unique binary/tri- Meta structure Chinese parasol tree mutually cooperates with the characteristics of making layer: macropore provides efficient proton transport place, can substantially reduce diffusional resistance, mesoporous can Proton transmitting channel is served as, and micropore and/or mesoporous can be to improve the degree of scatter of reactive material, and provide enough activity Center.Research confirms that these characteristics have porous carbon material and turn the incomparable excellent properties of system porous material, for example, Efficient chemical clean property surface, quick mass transfer rate and extremely short diffusion length etc., therefore, porous carbon material is in letterization, suction The fields such as attached, separation, biological medicine, strong energy have a wide range of applications.
Currently, the method for production of porous carbon material has template, template-activation combination method or exempts from template, they Preparing raw material and one Yin of template will can just be obtained by a series of cumbersome chemical reactions, certainly will be needed during this consume and More industrial chemicals is wasted, the energy is caused to waste and pollutes environment.
Summary of the invention
The present invention provides a kind of porous carbon fiber material, prepares level hole carbon material process wave in the prior art to solve Take the defect of the energy.
In order to overcome the defect of above-mentioned background technique, the present invention provides a kind of preparation method of porous carbon fiber material, The following steps are included:
Step S1: 6-8h is impregnated with sodium chloride solution after draft fasciated fiber is cleaned；
Step S2: the draft fasciated fiber for impregnating superchlorination sodium solution is transferred quickly in retort, is protected in inert atmosphere 680 DEG C -880 DEG C are warming up to the heating rate of 4-6 DEG C/min under shield, then constant temperature 6.5-7h is carbonized, and obtains carbon fiber Material, specific surface area 32-587m2/g；
Step S3: the resulting carbon fibre material merging of step S2 equipped with heating oil and is filled in the pressure pan of inert atmosphere It impregnates, heating oil is then warming up to 150 DEG C -230 DEG C, constant temperature 1-3h, while pressure pan with the heating rate of 6-10 DEG C/min Rotation；
Step S4: will the resulting carbon fibre material of step S3 take out after be placed in high temperature furnace, under inert atmosphere protection with The heating rate of 8-14 DEG C/min is warming up to 750 DEG C -880 DEG C, and then constant temperature 3-5h carries out activation etching；
Step S5: etch product, to neutrality, obtains porous carbon fiber material through 60-90 DEG C of water washing.
Sodium chloride solution saturation degree is 78%-85% in step S1, and sodium chloride solution temperature is 60 DEG C -75 DEG C.
A kind of preparation method of more high specific surface area porous Carbon fibe material, specific surface area 832-3835m2/ g, Microwave Field Heating is used in step S4, sprays high-pressure steam to carbon fibre material in 1/3 and 2/3 timing node of heating.
The high-pressure steam temperature is 100-160 DEG C, and high-pressure steam injecting time is 10-30min.
Step S2, the inert atmosphere in S4 is nitrogen or helium.
On the basis of step S3, the present invention provides a kind of pressure pans for being used to prepare porous carbon fiber material, including Tank body and liner, tank body upper end sealed set cover, liner at the bottom is connect with tank base by shaft and sealed set, liner Top is connect with tank wall by bearing and sealed set, and outer race is fixedly connected with inner tank wall, bearing inner ring with it is interior Gall bladder wall is fixedly connected.
In order to make to be filled with inert gas in liner, preferred technical solution is that cavity, liner are formed between liner and tank body Nozzle is arranged in inner wall, and nozzle is arranged towards liner center position, and nozzle is connected with cavity, and air inlet pipe, air inlet is arranged in tank base Pipe connects inertia gas tank, and air inlet pipe is connected with cavity, and relief valve is arranged on cover.
In order to enable liner to rotate in tank body, preferred technical solution is, straight where nozzle spray direction and nozzle Angle is set between diameter, and nozzle inclination direction is consistent.
In order to which the gas for spraying nozzle is able to drive liner rotation, preferred technical solution is, shaft is to inside liner Extend, protrude into the shaft side setting flabellum of liner, nozzle is sprayed towards flabellum direction.
Even closer in order to cooperate cover and tank body, preferred technical solution is uniformly to set at tank body upper end opening Several pedestals are set, locking level is hingedly set on each pedestal, may be stuck on cover after locking level rotation, locking level is close to pedestal Drive rod is arranged in the outside of one end, and tank wall corresponds to drive rod bottom end setting telescopic rod, and drive rod bottom end is arranged strip hole, stretches The telescopic end of contracting bar and strip hole are hinged；Location hole, cover top is arranged towards the side of cover center position in locking level top Locating ring is set, and locating ring lateral surface corresponds to position of positioning hole setting locating rod, and after locking level is stuck on cover, locating rod is inserted Enter in location hole.
The invention has the benefit that
The preparation method of porous carbon fiber material provided by the invention is base stock by using draft fasciated fiber, Charing obtains porous carbon fiber in inert atmosphere, avoids being fabricated to basic fibrous raw material using industrial chemicals, reduces chemical industry original The use of material, has saved the energy, avoids environmental pollution.
Other features and advantages of the present invention will be illustrated in the following description, also, partly becomes from specification It obtains it is clear that understand through the implementation of the invention.The objectives and other advantages of the invention can be by written explanation Specifically noted structure is achieved and obtained in book, claims and attached drawing.
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
A is the scanning electron microscope (SEM) photograph that porous carbon fiber material is made in the embodiment of the present invention 1 in Fig. 1；B is the embodiment of the present invention 2 The scanning electron microscope (SEM) photograph of porous carbon fiber material is made.
Fig. 2 is the side sectional view of the embodiment of the present invention 4；
Fig. 3 is the top view of the embodiment of the present invention 4；
Fig. 4 is cover partial schematic diagram in the embodiment of the present invention 4.
Wherein, 10- tank body；11- liner；12- cover；13- shaft；14- bearing；15- cavity；16- nozzle；17- air inlet Pipe；18- relief valve；19- flabellum；20- pedestal；21- locking level；22- drive rod；23- telescopic rod；24- strip hole；25- positioning Hole；26- locating ring；27- locating rod.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1
The present invention provides a kind of preparation methods of porous carbon fiber material, comprising the following steps:
Step S1: 7h is impregnated with sodium chloride solution after draft fasciated fiber is cleaned, herbaceous stem can be ramie, hemp, flax With the stem of jute；
Step S2: the draft fasciated fiber for impregnating superchlorination sodium solution is transferred quickly in retort, is protected in inert atmosphere 750 DEG C are warming up to the heating rate of 5 DEG C/min under shield, then constant temperature 6.8h is carbonized, and obtains carbon fibre material, compares table Area is 375m2/g；
The surface sweeping Electronic Speculum of level hole same feeling fibrous material made from above step is as shown in figure 1 shown in A.
Increase the toughness of draft fasciated fiber.
Embodiment 2
A kind of preparation method of more high specific surface area porous Carbon fibe material, the specific steps are as follows:
Step S1: 7h is impregnated with sodium chloride solution after draft fasciated fiber is cleaned, herbaceous stem can be ramie, hemp, flax With the stem of jute；
Step S2: the draft fasciated fiber for impregnating superchlorination sodium solution is transferred quickly in retort, is protected in inert atmosphere 800 DEG C are warming up to the heating rate of 6 DEG C/min under shield, then constant temperature 7h is carbonized；
Step S3: the resulting carbon fibre material merging of step S2 equipped with heating oil and is filled in the pressure pan of inert atmosphere It impregnates, heating oil is then warming up to 200 DEG C, constant temperature 2h with the heating rate of 8 DEG C/min, while pressure pan rotates；
Step S4: will the resulting carbon fibre material of step S3 take out after be placed in high temperature furnace, under inert atmosphere protection with The heating rate of 12 DEG C/min is warming up to 820 DEG C, and then constant temperature 5h carries out activation etching；
Step S5: etch product, to neutrality, obtains porous carbon fiber material, specific surface area is through 90 DEG C of water washing 3427m2/g。
The surface sweeping Electronic Speculum of level hole same feeling fibrous material made from above step is as shown in figure 1 shown in B.
It is heated by heating oil, carbon fiber generates hole and blows the buffering for being heated oil, prevents carbon fiber excessive It is broken.
Embodiment 3
Microwave Field Heating is used in the step S4 of embodiment 2, heating 1/3 and 2/3 timing node to carbon fiber material Material injection high-pressure steam.
The high-pressure steam temperature is 100-160 DEG C, and high-pressure steam injecting time is 10-30min, final to arrive The specific surface area of porous carbon fiber material is 3727m2/g。
Sodium chloride solution saturation degree is 78%-85% in step S1, and sodium chloride solution temperature is 60 DEG C -75 DEG C.
Step S2, the inert atmosphere in S4 is nitrogen or helium.
By spraying high-pressure steam to carbon fibre material, so that the heating oil on carbon fiber is encountered vapor, generate explosion Effect increases the generation quantity of carbon fibre material hole.
Embodiment 4
As shown in Fig. 2, the present invention provides a kind of height for being used to prepare porous carbon fiber material on the basis of step S3 Tank, including tank body 10 and liner 11 are pressed, 10 upper end sealed set cover 12 of tank body, 11 bottom of liner and 10 bottom of tank body are by turning The connection of axis 13 and sealed set, 11 top of liner is connect with 10 side wall of tank body by bearing 14 and sealed set, 14 outer ring of bearing It is fixedly connected with 10 inner wall of tank body, 14 inner ring of bearing is fixedly connected with 11 outer wall of liner.
The working principle of above-mentioned technical proposal are as follows:
Heating oil is added first in liner 11, carbon fibre material merging is equipped with heating oil and is filled with the height of inert atmosphere It is impregnated in pressure tank, covers cover 12, the heating oil in tank body 10 is heated, liner 11 can pass through rotating electric machine band turn It is dynamic.
Above-mentioned technical proposal has the beneficial effect that
Heating oil is housed by carbon fibre material merging and is filled with immersion rotating electric machine in the pressure pan of inert atmosphere and is driven Liner 11 rotates, and then carbon fibre material is enable to be sufficiently mixed with heating oil.
As shown in Figure 2,3, in order to make to be filled with inert gas in liner 11, preferred technical solution is liner 11 and tank body Cavity 15 is formed between 10, nozzle 16 is arranged in 11 inner wall of liner, and nozzle 16 is arranged towards 11 center position of liner, nozzle 16 and sky Chamber 15 is connected, and air inlet pipe 17 is arranged in 10 bottom of tank body, and air inlet pipe 17 connects inertia gas tank, and air inlet pipe 17 and cavity 15 are connected, tank Relief valve 18 is set on lid 12.
In order to enable liner 11 to rotate in tank body 10, preferred technical solution is 16 injection direction of nozzle and nozzle Angle is set between 16 place diameters, and 16 inclined direction of nozzle is consistent.
It is rotated in order to which the gas for spraying nozzle 16 is able to drive liner 11, preferred technical solution is that shaft 13 is inside 11 internal stretch of gallbladder, protrudes into 13 side of the shaft setting flabellum 19 of liner 11, and nozzle 16 is sprayed towards 19 direction of flabellum.
It the working principle of above-mentioned technical proposal and has the beneficial effect that
Inert gas is filled with into cavity 15 by air inlet pipe 17, then high-pressure inert gas passes through nozzle 16 to flabellum 19 It sprays, high-pressure inert gas is blown on flabellum 19, gives 11 recoil strength of liner, while cooperating flabellum 19 fixed, gives heating oil Agitation force is brought, and then heating oil is enable sufficiently to heat to carbon fibre material, the carbon fibre material after heating adds in microwave field Heat sprays water in heating process on carbon fibre material, keeps layer of carbon fiber material secondary aperture richer.
As shown in figure 4, even closer in order to cooperate cover 12 and tank body 10, preferred technical solution is tank body 10 It is uniformly arranged several pedestals 20 at upper end opening, locking level 21 is hingedly set on each pedestal 20, locking level 21 is inverted L Type, locking level 21 may be stuck on cover 12 after rotating, and drive rod 22, tank body is arranged close to the outside of 20 one end of pedestal in locking level 21 10 side walls correspond to 22 bottom end of drive rod setting telescopic rod 23, and strip hole 24, the telescopic end of telescopic rod 23 is arranged in 22 bottom end of drive rod It is hinged with strip hole 24；Location hole 25 is arranged towards the side of 12 center position of cover in 21 top of locking level, and 12 top of cover is set Locating ring 26 is set, 26 lateral surface of locating ring corresponds to 25 position of location hole setting locating rod 27, when locking level 21 is stuck on cover 12 Afterwards, locating rod 27 is inserted into location hole 25.
The working principle of above-mentioned technical proposal are as follows:
Telescopic rod 23 stretches out, and the telescopic end of telescopic rod 23 slides in strip hole 24, and the telescopic end of telescopic rod 23 pushes lock Fixed pole 21 rotates, and locking level 21 pushes down cover 12, and the location hole 25 on locking level 21 is inserted into the locating rod 27 on locating ring 26 On.
Above-mentioned technical proposal has the beneficial effect that
It is stretched out by telescopic rod 23, the telescopic end of telescopic rod 23 slides in strip hole 24, and the telescopic end of telescopic rod 23 pushes away Dynamic locking level 21 rotates, and locking level 21 pushes down cover 12, and the location hole 25 on locking level 21 is inserted into the positioning on locating ring 26 On bar 27, cooperates cover 12 with tank body 10 tighter, the heating oil in tank body 10 is prevented to be boiling over.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies Within, then the present invention is also intended to include these modifications and variations.

Claims (10)

1. a kind of preparation method of porous carbon fiber material, which comprises the following steps:
Step S1: 6-8h is impregnated with sodium chloride solution after draft fasciated fiber is cleaned；
Step S2: the draft fasciated fiber for impregnating superchlorination sodium solution is transferred quickly in retort, under inert atmosphere protection 680 DEG C -880 DEG C are warming up to the heating rate of 4-6 DEG C/min, then constant temperature 6.5-7h is carbonized, and obtains carbon fibre material；
Step S3: the resulting carbon fibre material merging of step S2 is equipped with heating oil and is filled in the pressure pan of inert atmosphere and is soaked Then heating oil is warming up to 150 DEG C -230 DEG C, constant temperature 1-3h with the heating rate of 6-10 DEG C/min by bubble, while pressure pan revolves Turn；
Step S4: it is placed in high temperature furnace after the resulting carbon fibre material of step S3 is taken out, with 8-14 under inert atmosphere protection DEG C/heating rate of min is warming up to 750 DEG C -880 DEG C, then constant temperature 3-5h carries out activation etching；
Step S5: etch product, to neutrality, obtains porous carbon fiber material through 60-90 DEG C of water washing.
2. a kind of preparation method of porous carbon fiber material as described in claim 1, which is characterized in that sodium chloride in step S1 Solution saturation degree is 78%-85%, and sodium chloride solution temperature is 60 DEG C -75 DEG C.
3. a kind of preparation method of porous carbon fiber material as described in claim 1, which is characterized in that using micro- in step S4 Wave field heating sprays high-pressure steam to carbon fibre material in 1/3 and 2/3 timing node of heating.
4. a kind of preparation method of porous carbon fiber material as claimed in claim 3, which is characterized in that the high-pressure steam Temperature is 100-160 DEG C, and high-pressure steam injecting time is 10-30min.
5. a kind of preparation method of porous carbon fiber material as described in claim 1, which is characterized in that step S2, in S4 Inert atmosphere is nitrogen or helium.
6. a kind of pressure pan for being used to prepare porous carbon fiber material, which is characterized in that including tank body (10) and liner (11), tank Body (10) upper end sealed set cover (12), liner (11) bottom are connect and are sealed by shaft (13) with tank body (10) bottom and set It sets, liner (11) top is connect with tank body (10) side wall by bearing (14) and sealed set, bearing (14) outer ring and tank body (10) inner wall is fixedly connected, and bearing (14) inner ring is fixedly connected with liner (11) outer wall.
7. a kind of pressure pan for being used to prepare porous carbon fiber material as claimed in claim 6, which is characterized in that liner (11) Cavity (15) are formed between tank body (10), nozzle (16) are arranged in liner (11) inner wall, and nozzle (16) is towards liner (11) center Direction setting, nozzle (16) and cavity (15) are connected, and air inlet pipe (17) are arranged in tank body (10) bottom, and air inlet pipe (17) connects inertia Gas tank, air inlet pipe (17) and cavity (15) are connected, and relief valve (18) are arranged on cover (12).
8. a kind of pressure pan for being used to prepare porous carbon fiber material as claimed in claim 7, which is characterized in that nozzle (16) Angle is set between diameter where injection direction and nozzle (16), nozzle (16) inclined direction is consistent.
9. a kind of pressure pan for being used to prepare porous carbon fiber material as claimed in claim 8, which is characterized in that shaft (13) To liner (11) internal stretch, shaft (13) side setting flabellum (19) of liner (11) is protruded into, nozzle (16) is towards flabellum (19) Direction injection.
10. a kind of pressure pan for being used to prepare porous carbon fiber material as claimed in claim 6, which is characterized in that tank body (10) it is uniformly arranged at upper end opening several pedestals (20), hingedly setting locking level (21), locking level on each pedestal (20) (21) it may be stuck on cover (12) after rotating, drive rod (22) are arranged close to the outside of pedestal (20) one end in locking level (21), tank Body (10) side wall corresponds to drive rod (22) bottom end setting telescopic rod (23), and strip hole (24) are arranged in drive rod (22) bottom end, stretches The telescopic end of bar (23) and strip hole (24) are hinged；Locking level (21) top is fixed towards the setting of the side of cover (12) center position Locating ring (26) are arranged in position hole (25), cover (12) top, and it is fixed that locating ring (26) lateral surface corresponds to the setting of location hole (25) position Position bar (27), after locking level (21) is stuck on cover (12), locating rod (27) is inserted into location hole (25).
CN201910268603.2A 2019-04-04 2019-04-04 A kind of porous carbon fiber material and its preparation method and application Withdrawn CN110004522A (en)

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Application Number Priority Date Filing Date Title
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000303266A (en) * 1999-04-22 2000-10-31 Hidetaka Kato Porous carbon fiber material and reutilization of plant scraps
CN1736859A (en) * 2005-08-15 2006-02-22 昆明理工大学 Super active carbon preparation method
CN101332992A (en) * 2008-07-31 2008-12-31 福建师范大学 Method for preparing tung cell-based active carbon by zinc chloride chemical activation method
CN102505187A (en) * 2011-09-29 2012-06-20 中山大学 Hierarchical porosity carbon fiber material, preparation method and application thereof
CN204017754U (en) * 2014-07-02 2014-12-17 四川省汇泉罐头食品有限公司 A kind of agitator of canned food mixer
CN106006637A (en) * 2016-05-20 2016-10-12 佛山市聚成生化技术研发有限公司 Jackfruit shell odor adsorbing agent
CN106540655A (en) * 2015-09-22 2017-03-29 云南民族大学 A kind of method that microwave and the composite modified coffee shell of activator prepare formaldehyde adsorbent

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000303266A (en) * 1999-04-22 2000-10-31 Hidetaka Kato Porous carbon fiber material and reutilization of plant scraps
CN1736859A (en) * 2005-08-15 2006-02-22 昆明理工大学 Super active carbon preparation method
CN101332992A (en) * 2008-07-31 2008-12-31 福建师范大学 Method for preparing tung cell-based active carbon by zinc chloride chemical activation method
CN102505187A (en) * 2011-09-29 2012-06-20 中山大学 Hierarchical porosity carbon fiber material, preparation method and application thereof
CN204017754U (en) * 2014-07-02 2014-12-17 四川省汇泉罐头食品有限公司 A kind of agitator of canned food mixer
CN106540655A (en) * 2015-09-22 2017-03-29 云南民族大学 A kind of method that microwave and the composite modified coffee shell of activator prepare formaldehyde adsorbent
CN106006637A (en) * 2016-05-20 2016-10-12 佛山市聚成生化技术研发有限公司 Jackfruit shell odor adsorbing agent

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Application publication date: 20190712